CN103940800A - Laser confocal Brillouin-Raman spectral measurement method and apparatus - Google Patents
Laser confocal Brillouin-Raman spectral measurement method and apparatus Download PDFInfo
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Abstract
The invention belongs to the technical field of microscopic imaging and spectral measurement and relates to a high resolution spectral imaging and detection method and apparatus which combine confocal microscopic technology and spectral detection technology together, realize integration of images and spectrums and are used for three dimensional morphology reconstruction and micro-area morphological performance parameter measurement of a variety of samples. The method and apparatus utilize Rayleigh light abandoned by a traditional confocal Raman system and confocal technology for detection of the position of a sample, employs a spectral detection system for spectral detection and uses Brillouin diffusion light abandoned by a traditional confocal Raman detection technology to test properties like elasticity and piezoelectricity of a material, thereby realizing measurement of micro-area high spatial resolution morphological parameters of a sample. The method and apparatus provided by the invention have the advantages of accurate positioning, high spatial resolution, high spectral detection sensitivity, controllable measured spot size, etc. and have wide application prospects in fields like biomedicine, evidence collection of court, micro and nano-fabrication, material engineering, engineering physics, precise metering and physical chemistry.
Description
Technical field
The invention belongs to microspectrum technical field of imaging, confocal microscopy is combined with spectrographic detection technology, relate to a kind of confocal laser Brillouin-method for measuring Raman spectrum and device, can be used for the performance parameter combined test of microcell form and the high-resolution imaging of sample.
Technical background
Confocal laser Raman spectrum measuring technology is the new technology that Microbeam Analysis Techniques and Raman spectrum analysis technology are combined, it focuses on incident laser on sample by microscope, thereby can be in the situation that not disturbed by ambient substance, obtain the molecular structure etc. of product microcell in the same old way, be called as molecular probe.It not only can the same aspect of observing samples in the raman spectral signal of different microcells, can also distinguish the Raman signal of the every aspect that in observing samples, the degree of depth is different, sample is carried out to tomoscan, thereby be issued to the effect of carrying out " optical section " in the situation of not damaging sample.Confocal laser Raman spectrum measuring technology, due to its harmless spectrum tomography ability and high resolving power, has been widely used in the fields such as physics, chemistry, biomedicine, petrochemical complex, environmental science, material science, geology, criminal investigation and jewelry.
At present, the principle of typical confocal laser Raman spectrum detection instrument as shown in Figure 1, laser, after light path condenser focusing successively, pin hole, collimation lens, polarization splitting prism, quarter-wave plate, object lens, focuses on sample, inspires the Raman diffused light that is loaded with sample spectra characteristic; Mobile sample, the Raman diffused light that makes corresponding sample zones of different, again by quarter-wave plate and be polarized Amici prism and reflect, enters confocal Raman spectra detection system and carries out spectrographic detection.
There is following problem in existing confocal laser Raman spectrum detection instrument: 1, in order to reduce the energy loss of Raman diffused light, the pin hole of choosing in system is conventionally between 150 μ m～200 μ m, system utilizes photon excited to carry out focus location, pinhole size directly affects the halfwidth of confocal axial location curve, pinhole size causes more greatly system Focus accuracy to reduce, and reduces spatial resolution; 2, utilize faint Raman diffused light to position, reduced the sensitivity of system; 3,, in long-time spectrographic detection process, system is affected by the factors such as environment easily to drift about, produce out of focus, reduction system space resolving power; 4, system is carried out spectrographic detection only, and pattern is single.Above-mentioned reason has limited the ability of confocal Raman spectra microscopic system detection microscopic spectrum, has restricted further developing of crs technique.
In addition, existing confocal laser Raman spectrum detection instrument has also abandoned and has contained the Brillouin scattering spectrum that enriches sample message, make aspect the property detections such as its elasticity at material and piezoelectricity limited, measurement demand when having restricted mechanical form performance parameter.
Based on above-mentioned situation, the present invention proposes to abandon in sample scattering light that confocal detection system utilizes existing confocal Raman spectra detection system to collect is better than sample Raman diffused light 10
3～10
6rayleigh light beam doubly carries out detected with high accuracy, utilize the Brillouin scattering spectrum abandoning to test aspects such as the elasticity of sample, piezoelectricity, itself and Raman spectrum detection system are organically blended, to realizing the confocal Brillouin-Raman spectrum imaging of high-space resolution and detection, and the spectrographic detection of the realizing high spatial resolution micro-field tests problem demanding prompt solution that is current spectrum has extremely important theory and learning value.
Summary of the invention
The object of the invention is: in order to overcome existing confocal Raman spectra Detection Techniques spatial resolution, be difficult to improve and apply limited deficiency, propose a kind of confocal laser Brillouin-method for measuring Raman spectrum and device.
The concrete thought of patent of the present invention is: confocal laser technology and Raman spectrum Detection Techniques are organically combined, confocal system utilize systematic collection to sample scattering light in Rayleigh light beam the focus of focal beam spot carried out to real-time follow-up and locus survey, the elasticity of the Brillouin scattering spectrum that utilization is abandoned to sample, the aspects such as piezoelectricity are tested, Raman spectrum detection system utilize systematic collection to the scattered light of sample in Raman diffused light carry out spectrographic detection, and then by confocal detection system signal and Raman, Brillouin spectrum detection system signal organically blends, thereby realize, the high-space resolution of sample form performance parameter is surveyed.
The object of the invention is to be achieved through the following technical solutions.
Confocal laser Brillouin-method for measuring Raman spectrum of the present invention, to utilize dichroic optical system that Raman diffused light is separated from Reyleith scanttering light and Brillouin scattering, Reyleith scanttering light and Brillouin scattering enter confocal detection system through beam splitting system beam splitting rear portion and carry out focus location, another part enters Brillouin spectrum detection system and carries out Brillouin spectrum detection, Raman diffused light enters Raman spectrum detection system and carries out Raman spectrum detection, utilize accurate corresponding this characteristic in confocal curves maximal value M and focus O position, by maximizing, accurately catch the spectral information that excites hot spot focal position, realize the spectrographic detection of high-space resolution, the specific implementation step of the method is as follows:
1) by excitation beam generation system, produce exciting light, after the first beam splitting system, object lens, focus on sample, and inspire Reyleith scanttering light, be loaded with Raman diffused light and the Brillouin scattering of sample spectral characteristic;
2) mobile sample, make Raman diffused light, the Brillouin scattering of Reyleith scanttering light and corresponding sample zones of different again pass through object lens, and being reflexed to dichroic optical system by the first beam splitting system, dichroic optical system carries out separated by Raman diffused light with Reyleith scanttering light, Brillouin scattering;
3) Reyleith scanttering light and Brillouin scattering are entered the second beam splitting system by dichroic optical system reflection, Reyleith scanttering light and Brillouin scattering through the second beam splitting system transmission enter confocal detection system, utilize the first detector in confocal detection system, record the corresponding I (ν of intensity loudness of the concavo-convex variation of reflection sample, u), can carry out the test of three dimension scale tomography, wherein, v is horizontal normalization optical coordinate, and u is axial normalization optical coordinate;
4) Reyleith scanttering light and the Brillouin scattering through the second beam splitting system reflection enters Brillouin spectrum detection system, utilizes Brillouin spectrum detection system to record to be loaded with the brillouin scattering signal I (λ of sample characteristic
b), can carry out Brillouin spectrum test, wherein λ
bfor Brillouin light spectrum wavelength;
5) Raman diffused light enters Raman spectrum detection system through dichroic optical system transmission, utilizes Raman spectrum detection system to record to be loaded with the Raman scattering signal I (λ of sample characteristic
r), can carry out Raman spectrum test, wherein λ
rfor Raman spectrum wavelength;
6) by I (ν, u), I (λ
r) and I (λ
b) deliver to data processing module 11 and process, thereby obtain, comprise sample positional information I (ν, u) and spectral information I (λ
r), I (λ
b) three-dimensional measurement information I (ν, u, λ
r, λ
b);
7) make sample along x, y scanning direction, object lens scan in the z-direction, repeat above-mentioned steps and record near individual positional information I (ν, u) and the spectral information I (λ of comprising of one group of i of homologue mirror foci position
r), I (λ
b) sequence measuring information { I
i(λ
r, λ
b), I
i(ν, u) };
8) utilize distinguishable region δ
icorresponding positional information I
i(ν, u), finds out corresponding δ
ithe spectral information I in region
i(λ
r, λ
b) value, then according to the relation of v and lateral attitude coordinate (x, y) and the relation of u and axial location coordinate z, reconstruct reflection measured object microcell δ
ithe information I of three dimension scale and spectral characteristic
i(x
i, y
i, z
i, λ
ri, λ
bi), realized microcell δ
minspectrographic detection and three-dimensional geometry position sensing;
9) corresponding minimum distinguishable region δ
minthree dimension scale and spectral characteristic by following formula, determined:
The confocal Brillouin of high-space resolution, Raman spectrum detection have been realized.
In detection method of the present invention, the homologue mirror foci O of confocal curves maximal value M place, focused spot size is minimum herein, the region of surveying is minimum, the out of focus region of the corresponding object lens in other positions of confocal curves, and the focused spot size before burnt or in defocused BB' region increases with defocusing amount, utilize this feature, z by adjusting sample is to defocusing amount, and according to Surveying Actual Precision demand, controls the size of focal beam spot, can realize sample search coverage size controlled.
In detection method of the present invention, excitation beam can be light beam: line polarisation, rotatory polarization, radial polarisation light etc.; Can also be the structure light beam being generated by pupil filtering technology, itself and polarization Modulation coupling can be compressed measurement focused spot size, improve system transverse resolution.
The invention provides a kind of confocal laser Brillouin-raman spectroscopy measurement device, comprise that excitation beam produces system, the first beam splitting system, object lens, 3 D scanning system, dichroic optical system, Raman spectrum detection system, the second beam splitting system, Brillouin spectrum detection system, confocal detection system and data processing module, wherein, the first beam splitting system, object lens, 3 D scanning system is placed on along light path the exit direction that excitation beam produces system successively, dichroic optical system is positioned at the reflection direction of the first beam splitting system, Raman spectrum detection system is positioned at the transmission direction of dichroic optical system, the second beam splitting system is positioned at the reflection direction of dichroic optical system, Brillouin spectrum detection system is positioned at the reflection direction of the second beam splitting system, confocal detection system is positioned at the reflection direction of the second beam splitting system, data processing module and Raman spectrum detection system, Brillouin spectrum detection system is connected with confocal detection system, be used for merging and processing Raman spectrum detection system, the data that Brillouin spectrum detection system and confocal detection system collect.
In device of the present invention, spectrum investigating system can be common Raman, Brillouin spectrum detection system, comprise the 3rd condenser placed successively along light path, be positioned at the Raman spectrometer of the 3rd condenser focal position and be positioned at the second detector after Raman spectrometer, the 4th condenser of placing successively along light path, position the 4th Brillouin light spectrometer in condenser focal position and be positioned at the 3rd detector after Brillouin light spectrometer, for the top layer spectrographic detection of sample, it can also be confocal Raman, Brillouin spectrum detection system, comprise the 3rd condenser of placing successively along light path, be positioned at the 3rd pin hole of the 3rd condenser focal position, the 3rd is positioned at the 5th condenser after pin hole, be positioned at the Raman spectrometer after the 5th condenser and be positioned at the second detector after Raman spectrometer, the 4th condenser of placing successively along light path, be positioned at the 4th pin hole of the 4th condenser focal position, be positioned at the 6th condenser after the 4th pin hole, be positioned at the Brillouin light spectrometer after the 6th condenser and be positioned at the 3rd detector after Brillouin light spectrometer, be used for improving system signal noise ratio and spatial resolution, and the chromatography spectrographic detection to sample.
In device of the present invention, excitation beam produces system can also comprise light polarization modulator and iris filter, for generation of polarized light and structure light beam.
In device of the present invention, for compressing, excite the iris filter of hot spot can be between radial polarisation optical generator and the first beam splitting system, can also be between the first beam splitting system and object lens.
In device of the present invention, Brillouin spectrum detection system can also be placed on the transmission direction of the second beam splitting system, and confocal detection system is positioned at the reflection direction of the second beam splitting system.
In device of the present invention, excitation beam produces system can also put the reflection direction of the first beam splitting system, dichroic optical system is successively placed on the transmission direction of the first beam splitting system along light path, Raman spectrum detection system is positioned at the transmission direction of dichroic optical system, the second beam splitting system is positioned at the reflection direction of dichroic optical system, Brillouin spectrum detection system is positioned at the reflection direction of the second beam splitting system, confocal detection system is positioned at the transmission direction of the second beam splitting system, data processing module connects confocal detection system, Raman spectrum detection system and Brillouin spectrum detection system.
In device of the present invention, can also comprise three-beam-splitting system and be positioned at the microscopic observation system of three-beam-splitting system reflection direction, for sample, slightly take aim at; Wherein, three-beam-splitting system can produce between system and the first beam splitting system at excitation beam, can also be between the first beam splitting system and object lens.
In device of the present invention, data processing module comprises for the treatment of the confocal data module of positional information with for merging the data fusion module of positional information and spectral information.
Beneficial effect:
The present invention contrasts prior art and has following innovative point:
1) the present invention can survey containing raman scattering spectrum and the Brillouin scattering spectrum of different information by appropriate design simultaneously, form and have complementary advantages, realized material composition and the high-resolution of basic physical property have been surveyed, be convenient to the integration test of many performance parameters;
2) utilize the maximum of points and accurate corresponding this characteristic in focal position of confocal system axial response curve, by family curve maximum of points, accurately catch the spectral information that excites hot spot focal position, realize the spectrographic detection of high-space resolution;
3) utilize dichroic light-dividing device to systematic collection to Reyleith scanttering light and the Raman diffused light that is loaded with sample information carry out light splitting, Reyleith scanttering light enters confocal detection system, Raman diffused light enters Raman spectrum detection system, realize the utilization completely of luminous energy, what make that faint Raman diffused light can can't harm enters Raman spectrum detection system, improves system spectrum detection sensitivity;
4) confocal microscope system and Raman spectrum imaging system are merged mutually on 26S Proteasome Structure and Function, both can realize the tomography of sample microcell geometric parameter, the spectrographic detection of sample microcell be can realize again, three dimension scale tomography, collection of illustrative plates tomography and three kinds of imaging patterns of spectrum test realized simultaneously;
5) can be by the beam splitting system before confocal detection system and Brillouin spectrum detection system is selected to suitable saturating inverse ratio, with maximum using light intensity.
The present invention contrasts prior art and has following remarkable advantage:
1) merge confocal technology and spectrographic detection technology, utilize the accurate location of confocal system focusing, significantly improve the spatial resolution of spectrographic detection;
2) utilize the out of focus region of confocal response curve, regulation and control focused spot size, can meet different testing requirements, makes system have versatility;
3) system is taken into account microscale tomography, collection of illustrative plates tomography and three kinds of imaging patterns of spectrum test simultaneously.
Accompanying drawing explanation
Fig. 1 is confocal Raman spectra formation method schematic diagram;
Fig. 2 is confocal laser Brillouin-method for measuring Raman spectrum schematic diagram;
Fig. 3 is confocal laser Brillouin-raman spectroscopy measurement device schematic diagram;
Fig. 4 is confocal laser Brillouin-raman spectroscopy measurement device schematic diagram with confocal spectrographic detection function;
Fig. 5 is confocal laser Brillouin-raman spectroscopy measurement device schematic diagram that Brillouin spectrum transmission-type is surveyed;
Fig. 6 is the confocal Brillouin-raman spectroscopy measurement of excitation source reflective laser device schematic diagram;
Fig. 7 is confocal laser Brillouin-raman spectroscopy measurement device schematic diagram with microscopic function;
Fig. 8 is the confocal laser Brillouin-method for measuring Raman spectrum and device embodiment schematic diagram with microscopic function;
Wherein, 1-excitation beam produces system, 2-the first beam splitting system, 3-object lens, 4-sample, 5-3 D scanning system, 6-dichroic optical system, 7-Raman spectrum detection system, 8-the second beam splitting system, 9-Brillouin spectrum detection system, the confocal detection system of 10-, 11-data processing module, 12-Raman spectrum response curve, the confocal response curve of 13-, 14-Brillouin spectrum response curve, 15-the first condenser, 16-the first pin hole, 17-the first detector, 18-laser instrument, 19-second condenser lens, 20-the second pin hole, 21-the first collimation lens, 22-radial polarisation optical generator, 23-iris filter, 24-the 3rd condenser, 25-Raman spectrometer, 26-the second detector, 27-the 4th condenser, 28-Brillouin light spectrometer, 29-the 3rd detector, the confocal data module of 30-, 31-data fusion module, 32-the 3rd pin hole, 33-the 5th condenser, 34-the 4th pin hole, 35-the 6th condenser, 36-three-beam-splitting system, 37-microscopic observation system, 38-the 4th beam splitting system, 39-Kohler illumination system, 40-the 7th condenser, 41-the 4th detector, 42-entrance slit, 43-plane mirror, 44-the first concave reflection condenser, 45-spectrum grating, 46-the second concave reflection condenser, 47-exit slit, 48-the 5th pin hole, 49-the second collimation lens, the even angle prism of 50-first, the even angle prism of 51-second, the logical F-P of 52-more than first, the logical F-P of 53-more than second, 54-the 8th condenser, 55-the 6th pin hole, 56-quarter-wave plate.
Embodiment
Below in conjunction with drawings and Examples, the invention will be further described.
Basic thought of the present invention is to utilize confocal detection and confocal Raman detection to combine to realize the Raman spectrum of high-space resolution to survey, and utilizes Brillouin scattering to measure parameters such as the elasticity of sample, piezoelectricity.
As shown in Figure 2, excitation beam produces system 1 and produces exciting light, through the first beam splitting system 2, after object lens 3, focus on sample 4, and inspire Reyleith scanttering light and be loaded with Raman diffused light and the Brillouin scattering of sample 4 spectral characteristics, the Raman diffused light inspiring, Brillouin scattering and Reyleith scanttering light are by systematic collection recovering light path, after object lens 3, be polarized Amici prism 2 and reflex to dichroic optical system 6, after dichroic optical system 6 light splitting, Raman diffused light is separated from Reyleith scanttering light and Brillouin scattering, Reyleith scanttering light and Brillouin scattering enter the second beam splitting system 8 and carry out beam splitting, through the Reyleith scanttering light of the second beam splitting system 8 transmissions and Brillouin scattering, enter confocal detection system 10 and carry out position sensing, the Reyleith scanttering light reflecting through the second beam splitting system 8 and Brillouin scattering enter Brillouin spectrum detection system 9 and carry out Brillouin spectrum detection, through the Raman diffused light of dichroic optical system 6 transmissions, enter Raman spectrum detection system 7 and carry out Raman spectrum detection.
As shown in Figure 3, this device comprises that the excitation beam of placing successively along light path produces system 1, the first beam splitting system 2, object lens 3, sample 4, 3 D scanning system 5, the dichroic optical system 6 of the first beam splitting system 2 reflection directions, be positioned at the Raman spectrum detection system 7 of dichroic optical system 6 transmission direction, be positioned at the second beam splitting system 8 of dichroic optical system 6 reflection directions, be positioned at the Brillouin spectrum detection system 9 of the second beam splitting system 8 reflection directions, and the confocal detection system 10 that is positioned at the second beam splitting system 8 transmission direction, also comprise and connect Raman spectrum detection system 7, the data processing module 11 of Brillouin spectrum detection system 9 and confocal detection system 10.
Raman spectrum detection system 7 in Fig. 3 is replaced with to the confocal Raman spectra detection system that comprises the 3rd condenser 24, the 3rd pin hole 32, the 5th condenser 33, Raman spectrometer 25 and the second detector 26, Brillouin spectrum detection system 9 is replaced with to the confocal Brillouin spectrum detection system that comprises the 4th condenser 27, the 4th pin hole 34, the 6th condenser 35, Raman spectrometer 28 and the 3rd detector 29, as shown in Figure 4.
Brillouin spectrum detection system in Fig. 4 is positioned over to the transmission direction of the second beam splitting system 8, confocal detection system 10 is positioned over the reflection direction of the second beam splitting system 8, and pie graph 5.
Excitation beam in Fig. 4 is produced to the reflection direction that system 1 is positioned over the first beam splitting system 2, and dichroic optical system 6 is positioned over the transmission direction of the first beam splitting system 2, and pie graph 6.
Between polarization the first beam splitting system 2 and object lens 3, add three-beam-splitting system 36, the three-beam-splitting system 36 reflection directions and add microscopic observation system 37, pie graph 7.
Embodiment
In the present embodiment, the first beam splitting system 2 is polarization splitting prism, 3 D scanning system 5 is 3-D scanning worktable, dichroic optical system 6 is Notch filter, the second beam splitting system 8 is spectroscope, and Brillouin light spectrometer 28 is F-P interferometer, and three-beam-splitting system 36 is for protecting inclined to one side Amici prism, the 4th beam splitting system 38 is broadband Amici prism, and the 4th detector 41 is CCD.
As shown in Figure 6, confocal laser Brillouin-method for measuring Raman spectrum, its testing procedure is as follows:
First, Kohler illumination system 39 produces equal white light, white light sees through after broadband Amici prism 38, protected inclined to one side Amici prism 36 reflections, through object lens 3, focus on sample 4, white light is reflected back toward original optical path, after being reflected respectively by the inclined to one side Amici prism 36 of guarantor, broadband Amici prism 38 after object lens 3, after the 7th condenser 40, enter CCD41, by the image of observing in CCD41, sample 4 is slightly taken aim at, to determine that sample 4 needs the region of observation to carry out coarse positioning to sample 4.
Then, the light beam that laser instrument 18 sends enters the second pin hole 20 after second condenser lens 19 is assembled, after the first collimation lens 21, collimator and extender is directional light, after radial polarisation optical generator 22 and iris filter 23, enter after polarization splitting prism 2 transmissions, by object lens 3, forming compression hot spot focuses on sample 4, and inspire Reyleith scanttering light and be loaded with Raman diffused light and the Brillouin scattering of sample 4 spectral characteristics, sample 4 can be processed by strengthening the Raman enhancing technology such as Raman spectrum nano particle, to improve Raman scattering light intensity.
Mobile sample 4, make the Raman diffused light of Reyleith scanttering light and corresponding sample 4 zoness of different, Brillouin scattering is returned original optical path by systematic collection and entered object lens 3, after polarization splitting prism 2 reflections, enter Notch filter6, Notch filter6 is harmless separated with other spectrum by Raman diffused light, Raman diffused light through Notch filter6 transmission enters Raman spectrum detection system 7, Raman diffused light is assembled and is entered the rear arrival of the 3rd pin hole 32 the 5th convergent mirror 33 by the 3rd condenser 24, after being assembled by the 5th convergent mirror 33, enter Raman spectrometer 25, Raman diffused light is through entrance slit 42, after plane mirror 43 and the first concave reflection condenser 44 reflections, arrive spectrum grating 45, light beam is after spectrum grating 45 diffraction, by the second concave reflection condenser 46 reflect focalizations to exit slit 47, finally incide the second detector 26.Due to grating diffration effect, in Raman spectrum, the light of different wave length is separated from each other, from exit slit 47 light out, be monochromatic light, when spectrum grating 45 rotates, from the optical wavelength difference of exit slit 47 outgoing, by monitoring second response of detector 26 and the angle of grating rotating, can obtain the Raman spectrum of sample 4, Reyleith scanttering light and Brillouin scattering through Notch filter6 reflection enter spectroscope 8, Reyleith scanttering light and Brillouin scattering through spectroscope 8 reflections enter Brillouin spectrum detection system, comprise the 4th pin hole 34 that is positioned at the 4th condenser 27 focus places, be positioned at the 4th pin hole 34 the 6th condenser 35 afterwards, be positioned at the 6th condenser 35 after F-P interferometer 28, and be positioned at the 3rd detector 29 after F-P interferometer 28, wherein, F-P interferometer 28 comprises the 5th pin hole 48, the second collimation lens 49, the first even angle prism 50, the second even angle prism 51, logical F-P52 more than first, logical F-P53 more than second, the 8th condenser 54 and the 6th pin hole 55, Reyleith scanttering light and Brillouin scattering through spectroscope 8 transmissions enter confocal detection system 10, and light beam is received by the first detector 17 through the first condenser 15, after being positioned at the first pin hole 16 of the first condenser 15 focal positions.
In measuring process, by three-dimensional, sweep that 5 pairs of samples of worktable 4 carry out axially and during transversal scanning, the first detector 17 in confocal detection system 10, the intensity response that records the 4 concavo-convex variations of reaction sample is I (ν, u), by gained intensity response I (ν, u) being sent to confocal data module 11 processes, wherein, v is horizontal normalization optical coordinate, and u is axial normalization optical coordinate;
The Raman diffused light spectral signal that is loaded with sample 4 Raman spectral information that in Raman spectrum detection system 7, the second detector 26 detects is I (λ
r) (λ
rfor Raman spectrum wavelength);
The Brillouin scattering spectral signal that is loaded with sample 4 Brillouin light spectrum informations that in Brillouin spectrum detection system 9, the 3rd detector 29 detects is I (λ
b) (λ
bbrillouin light spectrum wavelength);
By I (λ
r), I (λ
b) and I (ν, u) be sent to data fusion module 30 and carry out data processing, thereby obtain, comprise sample 4 positional information I (ν, u) and spectral information I (λ
r, λ
b) three-dimensional measurement information I (ν, u, λ
r, λ
b).
Make sample 4 along x, y scanning direction, object lens 3 scan in the z-direction, repeat above-mentioned steps and record near individual positional information I (ν, u) and the spectral information I (λ of comprising of one group of i of homologue mirror foci position
r), I (λ
b) sequence measuring information { I
i(λ
r, λ
b), I
i(ν, u) };
Utilize distinguishable region δ
icorresponding positional information I
i(ν, u), finds out corresponding δ
ithe spectral information I in region
i(λ
r, λ
b) value, then according to the relation of v and lateral attitude coordinate (x, y) and the relation of u and axial location coordinate z, reconstruct reflection measured object microcell δ
ithe information I of three dimension scale and spectral characteristic
i(x
i, y
i, z
i, λ
ri, λ
bi), realized microcell δ
minspectrographic detection and three-dimensional geometry position sensing;
Corresponding minimum distinguishable region δ
minthree dimension scale and spectral characteristic by following formula, determined:
Can realize like this confocal Raman spectra of high-space resolution surveys.
As can be seen from Figure 8, by the maximum point of confocal detection system 10 response curves, can accurately catch the focal position that excites hot spot, from measuring sequence data { I
i(λ
r, λ
b), I
i(ν, u) } in, the excitation spectrum of extraction corresponding focus positions O, has realized microcell δ
minspectrographic detection and three-dimensional geometry position sensing.
By to metrical information { I
i(λ
r, λ
b), I
i(ν, u) } fusion treatment, can realize the multiple measurement pattern shown in above formula, that is: microcell collection of illustrative plates tomography test, microcell Raman spectrum tomography, microcell Brillouin spectrum tomography, three dimension scale tomography, Raman spectrum detection, Brillouin spectrum detection etc.
As shown in Figure 8, confocal laser Brillouin-raman spectroscopy measurement device comprises that the excitation beam that is positioned at polarization splitting prism 2 incident directions produces system 1, be positioned at the object lens 3 that polarization splitting prism 2 transmission direction are placed successively along light path, sample 4, 3-D scanning worktable 5 and be positioned at the Notch filter6 of polarization splitting prism 2 reflection directions, be positioned at the Raman spectrum detection system 7 of Notch filter6 transmission direction, be positioned at the spectroscope 8 of Notch filter6 reflection direction, be positioned at the Brillouin spectrum detection system of spectroscope 8 reflection directions, be positioned at the confocal detection system 10 of spectroscope 8 transmission direction, and be positioned at confocal detection system 10, the data processing module 11 of Raman spectrum detection system 7 and Brillouin spectrum detection system 9 junctions, wherein, excitation beam produces system 1 for generation of excitation beam, comprises along light path and places successively laser instrument 18, second condenser lens 19, is positioned at the second pin hole 20, the first collimation lens 21, radial polarisation optical generator 22 and the iris filter 23 of second condenser lens 19 focal positions, Raman spectrum detection system 7 comprises the 3rd condenser 24 placed successively along light path, is positioned at the 3rd condenser 24 focal positions the 3rd pin hole 32, focus is positioned at the 5th condenser 33 at the 3rd pin hole place, Raman spectrometer 25 after the 5th condenser 33, wherein Raman spectrometer 25 comprises entrance slit 42, plane mirror 43, the first concave reflection condenser 44, spectrum grating 45, the second concave reflection condenser 46 and the exit slit 47 of once placing along light path, Brillouin spectrum detection system, comprise the 4th condenser 27 of placing successively along light path, be positioned at the 4th pin hole 34 at the 4th condenser 27 focus places, be positioned at the 4th pin hole 34 the 6th condenser 35 afterwards, be positioned at the 6th condenser 35 after F-P interferometer 28, and be positioned at the 3rd detector 29 after F-P interferometer 28, wherein, F-P interferometer 28 comprises the 5th pin hole 48, even angle prism 51, more than the first logical F-P52 of the even angle prism 50, second of the second collimation lens 49, first, more than second logical F-P53, the 8th condenser 54 and the 6th pin holes 55, Reyleith scanttering light and Brillouin scattering through spectroscope 8 transmissions enter confocal detection system 10, and light beam is received by the first detector 17 through the first condenser 15, after being positioned at the first pin hole 16 of the first condenser 15 focal positions.Data processing module 11 comprises confocal data module 30 and data fusion module 31, the data that collect for fusion treatment.
Below by reference to the accompanying drawings the specific embodiment of the present invention is described; but these explanations can not be understood to limit scope of the present invention; protection scope of the present invention is limited by the claims of enclosing, and any change of carrying out on the claims in the present invention basis is all protection scope of the present invention.
Claims (10)
1. confocal laser Brillouin-method for measuring Raman spectrum, it is characterized in that: utilize dichroic optical system that Raman diffused light is separated from Reyleith scanttering light and Brillouin scattering, Reyleith scanttering light and Brillouin scattering enter confocal detection system through spectroscope beam splitting rear portion and carry out focus location, another part enters Brillouin spectrum detection system and carries out Brillouin spectrum detection, Raman diffused light enters Raman spectrum detection system and carries out Raman spectrum detection, utilize accurate corresponding this characteristic in confocal curves maximal value M and focus O position, by maximizing, accurately catch the spectral information that excites hot spot focal position, realize the spectrographic detection of high-space resolution, the specific implementation step of the method is as follows:
1) by excitation beam, produce system (1) and produce exciting light, after the first beam splitting system (2), object lens (3), focus on sample (4) upper, and inspire Reyleith scanttering light, be loaded with Raman diffused light and the Brillouin scattering of sample spectral characteristic;
2) mobile sample (4), make Raman diffused light, the Brillouin scattering of Reyleith scanttering light and corresponding sample zones of different again pass through object lens (3), and being reflexed to dichroic optical system (6) by the first beam splitting system (2), dichroic optical system (6) carries out separated by Raman diffused light with Reyleith scanttering light, Brillouin scattering;
3) Reyleith scanttering light and Brillouin scattering are entered the second beam splitting system (8) by dichroic optical system reflection, Reyleith scanttering light and Brillouin scattering through the second beam splitting system (8) transmission enter confocal detection system, utilize the detector (17) in confocal detection system, record the corresponding I (ν of intensity loudness of the concavo-convex variation of reflection sample, u), can carry out the test of three dimension scale tomography, wherein, v is horizontal normalization optical coordinate, and u is axial normalization optical coordinate;
4) Reyleith scanttering light and the Brillouin scattering through the second beam splitting system (8) reflection enters Brillouin spectrum detection system (9), utilizes Brillouin spectrum detection system (9) to record to be loaded with the brillouin scattering signal I (λ of sample (4) characteristic
b), can carry out Brillouin spectrum test, wherein λ
bfor Brillouin light spectrum wavelength;
5) Raman diffused light enters Raman spectrum detection system (7) through dichroic optical system transmission, utilizes Raman spectrum detection system (7) to record to be loaded with the Raman scattering signal I (λ of sample characteristic
r), can carry out Raman spectrum test, wherein λ
rfor Raman spectrum wavelength;
6) by I (ν, u), I (λ
r) and I (λ
b) deliver to data processing module (11) and process, thereby obtain, comprise sample positional information I (ν, u) and spectral information I (λ
r), I (λ
b) three-dimensional measurement information I (ν, u, λ
r, λ
b);
7) make sample (4) along x, y scanning direction, object lens (3) scan in the z-direction, repeat above-mentioned steps and record near individual positional information I (ν, u) and the spectral information I (λ of comprising of one group of i of homologue mirror foci position
r), I (λ
b) sequence measuring information { I
i(λ
r, λ
b), I
i(ν, u) };
8) utilize distinguishable region δ
icorresponding positional information I
i(ν, u), finds out corresponding δ
ithe spectral information I in region
i(λ
r, λ
b) value, then according to the relation of v and lateral attitude coordinate (x, y) and the relation of u and axial location coordinate z, reconstruct reflection measured object microcell δ
ithe information I of three dimension scale and spectral characteristic
i(x
i, y
i, z
i, λ
ri, λ
bi), realized microcell δ
minspectrographic detection and three-dimensional geometry position sensing;
9) corresponding minimum distinguishable region δ
minthree dimension scale and spectral characteristic by following formula, determined:
The confocal Brillouin of high-space resolution, Raman spectrum detection have been realized.
2. according to the confocal laser Brillouin-method for measuring Raman spectrum described in right 1, it is characterized in that: the homologue mirror foci O of confocal curves (13) maximal value M place, focused spot size is minimum herein, the region of surveying is minimum, the out of focus region of the corresponding object lens in other positions of confocal curves (13), focused spot size before burnt or in defocused BB' region increases with defocusing amount, utilize this feature, z by adjusting sample is to defocusing amount, and according to Surveying Actual Precision demand, control the size of focal beam spot, control sample search coverage size.
3. according to the confocal laser Brillouin-method for measuring Raman spectrum described in right 1, it is characterized in that: excitation beam comprises light beam, line polarisation, rotatory polarization or radial polarisation light; Can also be the structure light beam being generated by pupil filtering technology, itself and polarization Modulation coupling can be compressed measurement focused spot size, improve system transverse resolution.
4. confocal laser Brillouin-raman spectroscopy measurement device, is characterized in that: comprise that excitation beam produces system (1), the first beam splitting system (2), object lens (3), 3 D scanning system (5), dichroic optical system (6), Raman spectrum detection system (7), the second beam splitting system (8), Brillouin spectrum detection system (9), confocal detection system (10) and data processing module (11), wherein, the first beam splitting system (2), object lens (3), 3 D scanning system (5) is placed on along light path the exit direction that excitation beam produces system (1) successively, dichroic optical system (6) is positioned at the reflection direction of the first beam splitting system (2), Raman spectrum detection system (7) is positioned at the transmission direction of dichroic optical system (6), the second beam splitting system (8) is positioned at the reflection direction of dichroic optical system (6), Brillouin spectrum detection system (9) is positioned at the reflection direction of the second beam splitting system (8), confocal detection system (10) is positioned at the reflection direction of the second beam splitting system (8), data processing module (11) and Raman spectrum detection system (7), Brillouin spectrum detection system (9) is connected with confocal detection system (10), be used for merging and processing Raman spectrum detection system (7), the data that Brillouin spectrum detection system (9) and confocal detection system (10) collect.
5. according to the confocal laser Brillouin-raman spectroscopy measurement device described in right 4, it is characterized in that: spectrum investigating system can be common Raman, Brillouin spectrum detection system, comprise the 3rd condenser (24) of placing successively along light path, be positioned at the Raman spectrometer (25) of the 3rd condenser (24) focal position and be positioned at the second detector (26) after Raman spectrometer (25), the 4th condenser 27 of placing successively along light path, be positioned at the Raman spectrometer (28) of the 4th condenser 27 focal positions and be positioned at the 3rd detector (29) after Raman spectrometer (28), top layer spectrographic detection for sample, it can also be confocal Raman, Brillouin spectrum detection system, comprise the 3rd condenser (24) of placing successively along light path, be positioned at the 3rd pin hole (32) of the 3rd condenser (24) focal position, be positioned at the 5th condenser (33) after the 3rd pin hole (32), be positioned at Raman spectrometer (25) afterwards of the 5th condenser (33) and be positioned at the second detector (26) after Raman spectrometer (25), the 4th condenser (27) of placing successively along light path, be positioned at the 4th pin hole (34) of the 4th condenser (27) focal position, be positioned at the 6th condenser (35) after the 4th pin hole (34), be positioned at Brillouin light spectrometer (28) afterwards of the 6th condenser (35) and be positioned at the 3rd detector (29) after Brillouin light spectrometer (28), be used for improving system signal noise ratio and spatial resolution, and the chromatography spectrographic detection to sample.
6. according to the confocal laser Brillouin-raman spectroscopy measurement device described in right 4, it is characterized in that: excitation beam produces system (1) and comprises radial polarisation optical generator (22) and iris filter (23), for generation of polarized light and structure light beam.
7. according to the confocal laser Brillouin-raman spectroscopy measurement device described in right 6, it is characterized in that: for compressing, excite the iris filter (23) of hot spot can be positioned between radial polarisation optical generator (22) and the first beam splitting system (2), can also be positioned between the first beam splitting system (2) and object lens (3).
8. according to the confocal laser Brillouin-raman spectroscopy measurement device described in right 4, it is characterized in that: Brillouin spectrum sniffer (9) can also be placed on the transmission direction of the second beam splitting system (8), differential confocal sniffer (10) is positioned at the reflection direction of the second beam splitting system (8).
9. according to the confocal laser Brillouin-raman spectroscopy measurement device described in right 4, it is characterized in that: excitation beam produces the reflection direction that system (1) can also be placed on the first beam splitting system (2), dichroic optical system (6) is successively placed on the transmission direction of the first beam splitting system (2) along light path, Raman spectrum detection system (7) is positioned at the transmission direction of dichroic optical system (6), the second beam splitting system (8) is positioned at the reflection direction of dichroic optical system (6), Brillouin spectrum detection system (9) is positioned at the reflection direction of the second beam splitting system (8), confocal detection system (10) is positioned at the transmission direction of the second beam splitting system (8), data processing module (11) connects confocal detection system (10), Raman spectrum detection system (7) and Brillouin spectrum detection system (9).
10. according to the confocal laser Brillouin-raman spectroscopy measurement device described in right 4, it is characterized in that: can also comprise three-beam-splitting system (36) and be positioned at the microscopic observation system (37) of three-beam-splitting system (36) reflection direction, for sample, slightly take aim at; Wherein, three-beam-splitting system (36) can be positioned at excitation beam and produce between system (1) and the first beam splitting system (2), can also be positioned between the first beam splitting system (2) and object lens (3).
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